# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1431 data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 O2 Sb2 Si2' _chemical_formula_weight 684.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.704(2) _cell_length_b 14.043(3) _cell_length_c 10.889(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.57(3) _cell_angle_gamma 90.00 _cell_volume 1542.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1. _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.848 _exptl_absorpt_correction_type scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13007 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3028 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZOSMN _computing_data_reduction DENZOSMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1309P)^2^+26.8922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3028 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 0.502 _refine_ls_restrained_S_all 0.502 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.54346(3) 0.07992(2) 0.07994(3) 0.02119(16) Uani 1 1 d . . . Si1 Si 0.77816(13) 0.14229(9) 0.41268(12) 0.0194(3) Uani 1 1 d . . . O1 O 0.7846(3) 0.0434(2) 0.3253(3) 0.0202(7) Uani 1 1 d . . . C1 C 0.7288(4) -0.0961(3) 0.1975(4) 0.0159(9) Uani 1 1 d . . . C2 C 0.6796(5) -0.1661(3) 0.2614(4) 0.0201(9) Uani 1 1 d . . . C3 C 0.7119(5) -0.2612(3) 0.2521(5) 0.0251(10) Uani 1 1 d . . . H3 H 0.6792 -0.3081 0.2966 0.030 Uiso 1 1 calc R . . C4 C 0.7904(5) -0.2897(3) 0.1799(5) 0.0263(11) Uani 1 1 d . . . C5 C 0.8355(5) -0.2194(4) 0.1143(5) 0.0249(10) Uani 1 1 d . . . H5 H 0.8867 -0.2378 0.0619 0.030 Uiso 1 1 calc R . . C6 C 0.8079(5) -0.1230(3) 0.1230(4) 0.0199(9) Uani 1 1 d . . . C7 C 0.5881(5) -0.1402(4) 0.3364(5) 0.0266(11) Uani 1 1 d . . . H7C H 0.5804 -0.1944 0.3901 0.032 Uiso 1 1 calc R . . H7B H 0.5003 -0.1240 0.2750 0.032 Uiso 1 1 calc R . . H7A H 0.6245 -0.0853 0.3926 0.032 Uiso 1 1 calc R . . C8 C 0.8632(6) -0.0502(4) 0.0527(5) 0.0294(11) Uani 1 1 d . . . H8C H 0.8999 -0.0828 -0.0072 0.035 Uiso 1 1 calc R . . H8B H 0.9334 -0.0136 0.1164 0.035 Uiso 1 1 calc R . . H8A H 0.7923 -0.0070 0.0033 0.035 Uiso 1 1 calc R . . C9 C 0.8283(7) -0.3941(4) 0.1738(6) 0.0394(14) Uani 1 1 d . . . H9C H 0.7912 -0.4169 0.0838 0.047 Uiso 1 1 calc R . . H9B H 0.7928 -0.4322 0.2300 0.047 Uiso 1 1 calc R . . H9A H 0.9251 -0.4000 0.2036 0.047 Uiso 1 1 calc R . . C10 C 0.6980(4) 0.0063(3) 0.2115(4) 0.0176(9) Uani 1 1 d . . . C11 C 0.9300(5) 0.1318(4) 0.5590(4) 0.0264(11) Uani 1 1 d . . . H11C H 1.0043 0.1103 0.5323 0.032 Uiso 1 1 calc R . . H11B H 0.9145 0.0856 0.6197 0.032 Uiso 1 1 calc R . . H11A H 0.9513 0.1940 0.6018 0.032 Uiso 1 1 calc R . . C12 C 0.6232(5) 0.1370(4) 0.4547(5) 0.0280(11) Uani 1 1 d . . . H12C H 0.6331 0.0891 0.5228 0.034 Uiso 1 1 calc R . . H12B H 0.5486 0.1197 0.3770 0.034 Uiso 1 1 calc R . . H12A H 0.6065 0.1994 0.4864 0.034 Uiso 1 1 calc R . . C13 C 0.7822(6) 0.2516(4) 0.3164(5) 0.0307(11) Uani 1 1 d . . . H13C H 0.7019 0.2542 0.2393 0.037 Uiso 1 1 calc R . . H13B H 0.8605 0.2498 0.2889 0.037 Uiso 1 1 calc R . . H13A H 0.7862 0.3081 0.3703 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0238(2) 0.0161(2) 0.0168(2) -0.00279(11) -0.00234(14) 0.00259(11) Si1 0.0208(7) 0.0187(6) 0.0154(6) -0.0029(5) 0.0018(5) -0.0008(5) O1 0.0197(17) 0.0210(16) 0.0150(15) -0.0041(13) -0.0005(13) -0.0009(13) C1 0.013(2) 0.018(2) 0.0110(19) -0.0043(16) -0.0033(17) -0.0005(16) C2 0.018(2) 0.021(2) 0.018(2) 0.0012(18) 0.0013(18) -0.0005(18) C3 0.026(3) 0.022(2) 0.021(2) 0.0005(19) -0.001(2) -0.006(2) C4 0.031(3) 0.022(2) 0.020(2) -0.0040(19) 0.001(2) 0.007(2) C5 0.017(2) 0.035(3) 0.019(2) -0.003(2) 0.0023(19) 0.004(2) C6 0.014(2) 0.022(2) 0.020(2) -0.0016(18) 0.0013(18) -0.0020(17) C7 0.027(3) 0.030(3) 0.026(2) 0.007(2) 0.013(2) 0.002(2) C8 0.035(3) 0.032(3) 0.027(3) 0.002(2) 0.017(2) -0.003(2) C9 0.051(4) 0.020(2) 0.037(3) -0.005(2) 0.003(3) 0.009(2) C10 0.015(2) 0.023(2) 0.014(2) -0.0004(17) 0.0041(17) -0.0015(17) C11 0.030(3) 0.026(2) 0.017(2) -0.0048(19) 0.000(2) -0.007(2) C12 0.022(3) 0.036(3) 0.026(2) -0.006(2) 0.007(2) 0.003(2) C13 0.035(3) 0.026(3) 0.024(2) 0.002(2) 0.000(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C10 2.066(5) . ? Sb1 Sb1 2.8018(8) 3_655 ? Si1 O1 1.697(3) . ? Si1 C11 1.862(5) . ? Si1 C12 1.864(5) . ? Si1 C13 1.868(5) . ? O1 C10 1.377(5) . ? C1 C2 1.405(6) . ? C1 C6 1.407(6) . ? C1 C10 1.495(6) . ? C2 C3 1.391(7) . ? C2 C7 1.515(6) . ? C3 C4 1.388(7) . ? C4 C5 1.396(7) . ? C4 C9 1.528(7) . ? C5 C6 1.396(7) . ? C6 C8 1.511(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Sb1 Sb1 92.99(13) . 3_655 ? O1 Si1 C11 103.1(2) . . ? O1 Si1 C12 108.1(2) . . ? C11 Si1 C12 112.4(2) . . ? O1 Si1 C13 110.2(2) . . ? C11 Si1 C13 111.6(2) . . ? C12 Si1 C13 111.1(3) . . ? C10 O1 Si1 132.3(3) . . ? C2 C1 C6 119.7(4) . . ? C2 C1 C10 119.4(4) . . ? C6 C1 C10 120.8(4) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C7 119.4(4) . . ? C1 C2 C7 121.0(4) . . ? C4 C3 C2 122.0(5) . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C9 121.4(5) . . ? C5 C4 C9 120.9(5) . . ? C6 C5 C4 122.3(4) . . ? C5 C6 C1 118.7(4) . . ? C5 C6 C8 119.6(4) . . ? C1 C6 C8 121.6(4) . . ? O1 C10 C1 110.6(4) . . ? O1 C10 Sb1 125.2(3) . . ? C1 C10 Sb1 124.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Si1 O1 C10 175.6(4) . . . . ? C12 Si1 O1 C10 56.4(4) . . . . ? C13 Si1 O1 C10 -65.2(4) . . . . ? C6 C1 C2 C3 1.2(7) . . . . ? C10 C1 C2 C3 -177.8(4) . . . . ? C6 C1 C2 C7 -176.7(4) . . . . ? C10 C1 C2 C7 4.3(7) . . . . ? C1 C2 C3 C4 -0.8(7) . . . . ? C7 C2 C3 C4 177.1(5) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C2 C3 C4 C9 178.2(5) . . . . ? C3 C4 C5 C6 2.2(7) . . . . ? C9 C4 C5 C6 -176.9(5) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? C4 C5 C6 C8 178.1(5) . . . . ? C2 C1 C6 C5 0.1(7) . . . . ? C10 C1 C6 C5 179.1(4) . . . . ? C2 C1 C6 C8 -179.9(4) . . . . ? C10 C1 C6 C8 -0.9(7) . . . . ? Si1 O1 C10 C1 -162.2(3) . . . . ? Si1 O1 C10 Sb1 16.2(6) . . . . ? C2 C1 C10 O1 82.8(5) . . . . ? C6 C1 C10 O1 -96.2(5) . . . . ? C2 C1 C10 Sb1 -95.7(5) . . . . ? C6 C1 C10 Sb1 85.3(5) . . . . ? Sb1 Sb1 C10 O1 -177.1(3) 3_655 . . . ? Sb1 Sb1 C10 C1 1.0(4) 3_655 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.484 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.106 #===end data_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H59 O2 Sb' _chemical_formula_weight 669.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z' 'x, y-1/2, -z-1/2' _cell_length_a 11.4906(2) _cell_length_b 20.0826(4) _cell_length_c 31.2742(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(2) _cell_angle_gamma 90.00 _cell_volume 7216.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min n/a _cell_measurement_theta_max n/a _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8574 _exptl_absorpt_correction_T_max 0.9249 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '1o phi frames, DX=30mm' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% 0 _diffrn_reflns_number 50378 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7003 _reflns_number_gt 5476 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+13.0156P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00099(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7003 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.329641(18) 0.371761(10) 0.128618(6) 0.01863(9) Uani 1 1 d . . . O1 O 0.1307(2) 0.37783(11) 0.19220(7) 0.0224(5) Uani 1 1 d . . . O2 O 0.07653(19) 0.40853(11) 0.11511(8) 0.0219(5) Uani 1 1 d . . . H2 H 0.090(5) 0.398(3) 0.1448(18) 0.080(17) Uiso 1 1 d . . . C1 C 0.2331(3) 0.35783(15) 0.18840(10) 0.0172(7) Uani 1 1 d . . . C2 C 0.2935(3) 0.32299(15) 0.22464(10) 0.0164(7) Uani 1 1 d . . . C3 C 0.3508(3) 0.36102(15) 0.25734(10) 0.0161(7) Uani 1 1 d . . . C4 C 0.4105(3) 0.32562(16) 0.28862(10) 0.0168(7) Uani 1 1 d . . . H4 H 0.4482 0.3502 0.3106 0.020 Uiso 1 1 calc R . . C5 C 0.4185(3) 0.25670(16) 0.28976(9) 0.0161(7) Uani 1 1 d . . . C6 C 0.3626(3) 0.22203(15) 0.25768(10) 0.0165(7) Uani 1 1 d . . . H6 H 0.3688 0.1749 0.2576 0.020 Uiso 1 1 calc R . . C7 C 0.2971(3) 0.25235(15) 0.22527(9) 0.0142(6) Uani 1 1 d . . . C8 C 0.3413(3) 0.43779(16) 0.26231(10) 0.0221(7) Uani 1 1 d . . . C9 C 0.3680(4) 0.47687(17) 0.22149(11) 0.0296(9) Uani 1 1 d . . . H9A H 0.3029 0.4724 0.2015 0.036 Uiso 1 1 calc R . . H9B H 0.4390 0.4593 0.2083 0.036 Uiso 1 1 calc R . . H9C H 0.3792 0.5240 0.2286 0.036 Uiso 1 1 calc R . . C10 C 0.2174(3) 0.45388(18) 0.27776(12) 0.0314(9) Uani 1 1 d . . . H10A H 0.2130 0.5009 0.2860 0.038 Uiso 1 1 calc R . . H10B H 0.1985 0.4260 0.3025 0.038 Uiso 1 1 calc R . . H10C H 0.1619 0.4450 0.2547 0.038 Uiso 1 1 calc R . . C11 C 0.4265(4) 0.46476(17) 0.29632(11) 0.0317(9) Uani 1 1 d . . . H11A H 0.5055 0.4495 0.2898 0.038 Uiso 1 1 calc R . . H11B H 0.4035 0.4484 0.3246 0.038 Uiso 1 1 calc R . . H11C H 0.4246 0.5135 0.2962 0.038 Uiso 1 1 calc R . . C12 C 0.4830(3) 0.22166(15) 0.32650(10) 0.0176(7) Uani 1 1 d . . . C13 C 0.4314(3) 0.24388(19) 0.36957(10) 0.0266(8) Uani 1 1 d . . . H13A H 0.4328 0.2926 0.3713 0.032 Uiso 1 1 calc R . . H13B H 0.4776 0.2251 0.3930 0.032 Uiso 1 1 calc R . . H13C H 0.3509 0.2281 0.3718 0.032 Uiso 1 1 calc R . . C14 C 0.6118(3) 0.24023(18) 0.32509(11) 0.0260(8) Uani 1 1 d . . . H14A H 0.6461 0.2239 0.2984 0.031 Uiso 1 1 calc R . . H14B H 0.6521 0.2200 0.3495 0.031 Uiso 1 1 calc R . . H14C H 0.6199 0.2888 0.3265 0.031 Uiso 1 1 calc R . . C15 C 0.4725(3) 0.14548(17) 0.32384(11) 0.0284(8) Uani 1 1 d . . . H15A H 0.3904 0.1327 0.3257 0.034 Uiso 1 1 calc R . . H15B H 0.5157 0.1252 0.3475 0.034 Uiso 1 1 calc R . . H15C H 0.5048 0.1300 0.2966 0.034 Uiso 1 1 calc R . . C16 C 0.2349(3) 0.20345(16) 0.19406(10) 0.0197(7) Uani 1 1 d . . . C17 C 0.1832(4) 0.14443(17) 0.21957(12) 0.0335(9) Uani 1 1 d . . . H17A H 0.2463 0.1192 0.2330 0.040 Uiso 1 1 calc R . . H17B H 0.1399 0.1152 0.2001 0.040 Uiso 1 1 calc R . . H17C H 0.1306 0.1615 0.2417 0.040 Uiso 1 1 calc R . . C18 C 0.3239(3) 0.1768(2) 0.16216(12) 0.0358(9) Uani 1 1 d . . . H18A H 0.3478 0.2126 0.1428 0.043 Uiso 1 1 calc R . . H18B H 0.2890 0.1405 0.1455 0.043 Uiso 1 1 calc R . . H18C H 0.3920 0.1600 0.1776 0.043 Uiso 1 1 calc R . . C19 C 0.1292(3) 0.23140(17) 0.17014(12) 0.0277(8) Uani 1 1 d . . . H19A H 0.0716 0.2474 0.1908 0.033 Uiso 1 1 calc R . . H19B H 0.0945 0.1963 0.1525 0.033 Uiso 1 1 calc R . . H19C H 0.1539 0.2684 0.1518 0.033 Uiso 1 1 calc R . . C20 C 0.1807(3) 0.40498(15) 0.09754(10) 0.0192(7) Uani 1 1 d . . . C21 C 0.1950(3) 0.43085(16) 0.05266(10) 0.0177(7) Uani 1 1 d . . . C22 C 0.2235(3) 0.38612(16) 0.01914(10) 0.0193(7) Uani 1 1 d . . . C23 C 0.2749(3) 0.41302(17) -0.01764(10) 0.0212(7) Uani 1 1 d . . . H23 H 0.2989 0.3832 -0.0395 0.025 Uiso 1 1 calc R . . C24 C 0.2926(3) 0.48024(17) -0.02388(10) 0.0197(7) Uani 1 1 d . . . C25 C 0.2489(3) 0.52301(16) 0.00727(10) 0.0185(7) Uani 1 1 d . . . H25 H 0.2524 0.5696 0.0021 0.022 Uiso 1 1 calc R . . C26 C 0.2003(3) 0.50106(15) 0.04570(10) 0.0167(7) Uani 1 1 d . . . C27 C 0.1957(3) 0.31020(16) 0.01831(10) 0.0229(8) Uani 1 1 d . . . C28 C 0.1044(3) 0.28808(17) 0.05082(11) 0.0297(8) Uani 1 1 d . . . H28A H 0.0359 0.3169 0.0486 0.036 Uiso 1 1 calc R . . H28B H 0.1370 0.2912 0.0797 0.036 Uiso 1 1 calc R . . H28C H 0.0819 0.2419 0.0450 0.036 Uiso 1 1 calc R . . C29 C 0.3084(3) 0.26952(18) 0.02477(12) 0.0316(9) Uani 1 1 d . . . H29A H 0.3367 0.2757 0.0541 0.038 Uiso 1 1 calc R . . H29B H 0.3678 0.2848 0.0045 0.038 Uiso 1 1 calc R . . H29C H 0.2923 0.2222 0.0198 0.038 Uiso 1 1 calc R . . C30 C 0.1452(4) 0.29183(18) -0.02566(11) 0.0335(9) Uani 1 1 d . . . H30A H 0.1133 0.2466 -0.0246 0.040 Uiso 1 1 calc R . . H30B H 0.2069 0.2939 -0.0473 0.040 Uiso 1 1 calc R . . H30C H 0.0833 0.3233 -0.0332 0.040 Uiso 1 1 calc R . . C31 C 0.3564(3) 0.50581(19) -0.06368(10) 0.0249(8) Uani 1 1 d . . . C32 C 0.4774(3) 0.4747(2) -0.06571(12) 0.0382(10) Uani 1 1 d . . . H32A H 0.5180 0.4907 -0.0913 0.046 Uiso 1 1 calc R . . H32B H 0.4702 0.4261 -0.0670 0.046 Uiso 1 1 calc R . . H32C H 0.5216 0.4872 -0.0402 0.046 Uiso 1 1 calc R . . C33 C 0.2877(4) 0.4874(2) -0.10404(11) 0.0393(10) Uani 1 1 d . . . H33A H 0.3220 0.5098 -0.1289 0.047 Uiso 1 1 calc R . . H33B H 0.2065 0.5015 -0.1007 0.047 Uiso 1 1 calc R . . H33C H 0.2907 0.4391 -0.1083 0.047 Uiso 1 1 calc R . . C34 C 0.3707(4) 0.5818(2) -0.06330(13) 0.0377(10) Uani 1 1 d . . . H34A H 0.4188 0.5949 -0.0389 0.045 Uiso 1 1 calc R . . H34B H 0.2940 0.6028 -0.0609 0.045 Uiso 1 1 calc R . . H34C H 0.4082 0.5962 -0.0899 0.045 Uiso 1 1 calc R . . C35 C 0.1497(3) 0.55441(16) 0.07664(10) 0.0198(7) Uani 1 1 d . . . C36 C 0.0159(3) 0.54790(17) 0.07641(11) 0.0251(8) Uani 1 1 d . . . H36A H -0.0128 0.5519 0.0470 0.030 Uiso 1 1 calc R . . H36B H -0.0181 0.5833 0.0940 0.030 Uiso 1 1 calc R . . H36C H -0.0063 0.5044 0.0881 0.030 Uiso 1 1 calc R . . C37 C 0.1788(3) 0.62593(16) 0.06171(11) 0.0290(8) Uani 1 1 d . . . H37A H 0.1449 0.6336 0.0334 0.035 Uiso 1 1 calc R . . H37B H 0.2635 0.6314 0.0602 0.035 Uiso 1 1 calc R . . H37C H 0.1465 0.6581 0.0821 0.035 Uiso 1 1 calc R . . C38 C 0.1971(3) 0.54979(17) 0.12284(10) 0.0248(8) Uani 1 1 d . . . H38A H 0.1678 0.5874 0.1396 0.030 Uiso 1 1 calc R . . H38B H 0.2823 0.5510 0.1223 0.030 Uiso 1 1 calc R . . H38C H 0.1711 0.5080 0.1359 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.01630(12) 0.02285(13) 0.01675(12) 0.00208(9) 0.00043(9) 0.00102(9) O1 0.0212(12) 0.0231(12) 0.0229(12) 0.0043(10) 0.0023(10) 0.0033(10) O2 0.0156(12) 0.0251(13) 0.0251(12) 0.0053(10) -0.0002(10) 0.0018(10) C1 0.0194(17) 0.0146(16) 0.0177(15) 0.0004(12) -0.0003(14) -0.0022(13) C2 0.0193(17) 0.0155(16) 0.0143(15) 0.0036(12) 0.0018(13) -0.0020(13) C3 0.0186(17) 0.0136(16) 0.0162(15) -0.0003(12) 0.0012(13) -0.0012(13) C4 0.0164(16) 0.0200(16) 0.0139(15) -0.0016(13) -0.0007(13) -0.0036(13) C5 0.0126(15) 0.0202(16) 0.0155(14) 0.0002(14) 0.0033(13) -0.0013(13) C6 0.0162(16) 0.0139(15) 0.0193(16) 0.0025(13) 0.0020(14) 0.0001(13) C7 0.0139(16) 0.0134(15) 0.0155(14) -0.0005(13) 0.0027(12) -0.0005(12) C8 0.030(2) 0.0148(16) 0.0213(17) 0.0016(13) -0.0027(16) -0.0029(15) C9 0.041(2) 0.0204(18) 0.0271(19) 0.0007(15) 0.0002(17) -0.0058(17) C10 0.041(2) 0.0192(18) 0.034(2) -0.0016(16) 0.0067(18) 0.0054(17) C11 0.050(2) 0.0154(17) 0.030(2) -0.0027(15) -0.0093(19) -0.0038(17) C12 0.0199(17) 0.0174(16) 0.0156(15) 0.0030(13) -0.0021(14) -0.0010(14) C13 0.0246(18) 0.036(2) 0.0191(16) 0.0052(16) -0.0015(16) 0.0069(16) C14 0.0199(18) 0.032(2) 0.0264(18) 0.0052(16) -0.0028(15) 0.0002(15) C15 0.032(2) 0.0249(19) 0.0281(19) 0.0068(15) -0.0088(17) 0.0011(16) C16 0.0210(18) 0.0166(16) 0.0216(16) -0.0046(13) -0.0037(15) 0.0003(14) C17 0.041(2) 0.0224(19) 0.037(2) 0.0037(16) -0.0129(19) -0.0091(17) C18 0.032(2) 0.041(2) 0.035(2) -0.0211(18) -0.0038(18) -0.0019(19) C19 0.0252(19) 0.0232(19) 0.035(2) 0.0000(15) -0.0082(16) -0.0062(15) C20 0.0219(17) 0.0144(15) 0.0212(16) -0.0002(13) 0.0006(14) -0.0042(14) C21 0.0131(17) 0.0214(17) 0.0186(16) 0.0002(13) -0.0024(13) 0.0015(13) C22 0.0196(16) 0.0204(17) 0.0179(16) -0.0020(13) -0.0028(14) 0.0045(14) C23 0.0205(17) 0.0262(18) 0.0170(16) -0.0067(14) -0.0008(14) 0.0054(15) C24 0.0159(17) 0.0273(18) 0.0161(16) 0.0016(14) -0.0040(13) 0.0006(14) C25 0.0167(17) 0.0203(17) 0.0185(15) 0.0052(13) -0.0045(14) -0.0006(13) C26 0.0159(17) 0.0170(16) 0.0174(16) 0.0040(13) 0.0000(13) 0.0010(13) C27 0.029(2) 0.0205(17) 0.0197(17) -0.0029(14) -0.0076(15) 0.0030(15) C28 0.035(2) 0.0238(19) 0.031(2) -0.0021(16) -0.0061(17) -0.0113(17) C29 0.037(2) 0.0257(19) 0.0317(19) -0.0040(16) -0.0085(18) 0.0085(17) C30 0.049(3) 0.0222(19) 0.030(2) -0.0051(16) -0.0135(19) 0.0005(17) C31 0.0209(18) 0.038(2) 0.0158(16) 0.0008(15) 0.0021(14) -0.0017(15) C32 0.031(2) 0.054(3) 0.030(2) 0.0025(19) 0.0096(18) 0.005(2) C33 0.034(2) 0.067(3) 0.0162(18) 0.0054(18) -0.0033(16) -0.011(2) C34 0.040(2) 0.042(2) 0.031(2) 0.0093(18) 0.0145(19) -0.0013(19) C35 0.0232(18) 0.0172(16) 0.0189(16) 0.0018(13) 0.0041(14) 0.0029(14) C36 0.0261(19) 0.0203(17) 0.0290(18) 0.0030(15) 0.0059(16) 0.0061(15) C37 0.040(2) 0.0168(16) 0.0298(19) -0.0013(15) 0.0100(17) 0.0035(17) C38 0.0297(19) 0.0228(17) 0.0221(18) -0.0054(14) 0.0052(15) 0.0014(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C20 2.078(3) . ? Sb1 C1 2.192(3) . ? O1 C1 1.248(4) . ? O2 C20 1.319(4) . ? C1 C2 1.502(4) . ? C2 C7 1.419(4) . ? C2 C3 1.436(4) . ? C3 C4 1.390(4) . ? C3 C8 1.553(4) . ? C4 C5 1.387(4) . ? C5 C6 1.380(4) . ? C5 C12 1.538(4) . ? C6 C7 1.402(4) . ? C7 C16 1.558(4) . ? C8 C9 1.530(5) . ? C8 C10 1.538(5) . ? C8 C11 1.544(5) . ? C12 C14 1.527(5) . ? C12 C15 1.537(4) . ? C12 C13 1.538(4) . ? C16 C18 1.526(5) . ? C16 C19 1.533(5) . ? C16 C17 1.547(5) . ? C20 C21 1.506(4) . ? C21 C22 1.419(4) . ? C21 C26 1.428(4) . ? C22 C23 1.401(5) . ? C22 C27 1.558(4) . ? C23 C24 1.379(5) . ? C24 C25 1.392(5) . ? C24 C31 1.533(4) . ? C25 C26 1.397(4) . ? C26 C35 1.556(4) . ? C27 C28 1.527(5) . ? C27 C30 1.538(5) . ? C27 C29 1.544(5) . ? C31 C32 1.525(5) . ? C31 C33 1.534(5) . ? C31 C34 1.535(5) . ? C35 C36 1.543(5) . ? C35 C38 1.547(4) . ? C35 C37 1.547(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Sb1 C1 91.32(12) . . ? O1 C1 C2 120.9(3) . . ? O1 C1 Sb1 121.1(2) . . ? C2 C1 Sb1 117.9(2) . . ? C7 C2 C3 120.6(3) . . ? C7 C2 C1 119.3(3) . . ? C3 C2 C1 120.1(3) . . ? C4 C3 C2 117.1(3) . . ? C4 C3 C8 118.1(3) . . ? C2 C3 C8 124.6(3) . . ? C5 C4 C3 124.1(3) . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C12 122.5(3) . . ? C4 C5 C12 120.5(3) . . ? C5 C6 C7 123.8(3) . . ? C6 C7 C2 117.4(3) . . ? C6 C7 C16 115.2(3) . . ? C2 C7 C16 127.4(3) . . ? C9 C8 C10 109.9(3) . . ? C9 C8 C11 105.5(3) . . ? C10 C8 C11 107.3(3) . . ? C9 C8 C3 114.3(3) . . ? C10 C8 C3 107.7(3) . . ? C11 C8 C3 111.9(3) . . ? C14 C12 C15 108.5(3) . . ? C14 C12 C13 109.2(3) . . ? C15 C12 C13 107.8(3) . . ? C14 C12 C5 109.5(3) . . ? C15 C12 C5 112.2(3) . . ? C13 C12 C5 109.6(3) . . ? C18 C16 C19 109.9(3) . . ? C18 C16 C17 109.0(3) . . ? C19 C16 C17 103.2(3) . . ? C18 C16 C7 108.9(3) . . ? C19 C16 C7 116.0(3) . . ? C17 C16 C7 109.6(3) . . ? O2 C20 C21 117.9(3) . . ? O2 C20 Sb1 124.7(2) . . ? C21 C20 Sb1 117.2(2) . . ? C22 C21 C26 120.2(3) . . ? C22 C21 C20 119.7(3) . . ? C26 C21 C20 119.2(3) . . ? C23 C22 C21 117.4(3) . . ? C23 C22 C27 116.8(3) . . ? C21 C22 C27 125.8(3) . . ? C24 C23 C22 123.8(3) . . ? C23 C24 C25 116.8(3) . . ? C23 C24 C31 120.9(3) . . ? C25 C24 C31 122.3(3) . . ? C24 C25 C26 123.5(3) . . ? C25 C26 C21 117.4(3) . . ? C25 C26 C35 117.9(3) . . ? C21 C26 C35 124.7(3) . . ? C28 C27 C30 105.4(3) . . ? C28 C27 C29 109.6(3) . . ? C30 C27 C29 107.9(3) . . ? C28 C27 C22 114.5(3) . . ? C30 C27 C22 109.1(3) . . ? C29 C27 C22 110.1(3) . . ? C32 C31 C24 109.4(3) . . ? C32 C31 C33 109.6(3) . . ? C24 C31 C33 109.9(3) . . ? C32 C31 C34 108.1(3) . . ? C24 C31 C34 112.2(3) . . ? C33 C31 C34 107.5(3) . . ? C36 C35 C38 110.5(3) . . ? C36 C35 C37 107.0(3) . . ? C38 C35 C37 105.2(3) . . ? C36 C35 C26 108.1(3) . . ? C38 C35 C26 114.1(3) . . ? C37 C35 C26 111.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 Sb1 C1 O1 -8.5(3) . . . . ? C20 Sb1 C1 C2 171.1(2) . . . . ? O1 C1 C2 C7 97.4(4) . . . . ? Sb1 C1 C2 C7 -82.2(3) . . . . ? O1 C1 C2 C3 -85.0(4) . . . . ? Sb1 C1 C2 C3 95.5(3) . . . . ? C7 C2 C3 C4 1.1(5) . . . . ? C1 C2 C3 C4 -176.5(3) . . . . ? C7 C2 C3 C8 -173.2(3) . . . . ? C1 C2 C3 C8 9.1(5) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C8 C3 C4 C5 175.3(3) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C3 C4 C5 C12 -177.9(3) . . . . ? C4 C5 C6 C7 -1.6(5) . . . . ? C12 C5 C6 C7 175.9(3) . . . . ? C5 C6 C7 C2 3.2(5) . . . . ? C5 C6 C7 C16 -176.2(3) . . . . ? C3 C2 C7 C6 -2.8(5) . . . . ? C1 C2 C7 C6 174.8(3) . . . . ? C3 C2 C7 C16 176.4(3) . . . . ? C1 C2 C7 C16 -5.9(5) . . . . ? C4 C3 C8 C9 133.8(3) . . . . ? C2 C3 C8 C9 -51.9(4) . . . . ? C4 C3 C8 C10 -103.7(3) . . . . ? C2 C3 C8 C10 70.5(4) . . . . ? C4 C3 C8 C11 13.9(4) . . . . ? C2 C3 C8 C11 -171.8(3) . . . . ? C6 C5 C12 C14 118.1(3) . . . . ? C4 C5 C12 C14 -64.5(4) . . . . ? C6 C5 C12 C15 -2.5(4) . . . . ? C4 C5 C12 C15 175.0(3) . . . . ? C6 C5 C12 C13 -122.2(3) . . . . ? C4 C5 C12 C13 55.2(4) . . . . ? C6 C7 C16 C18 -78.1(4) . . . . ? C2 C7 C16 C18 102.7(4) . . . . ? C6 C7 C16 C19 157.4(3) . . . . ? C2 C7 C16 C19 -21.9(5) . . . . ? C6 C7 C16 C17 41.1(4) . . . . ? C2 C7 C16 C17 -138.2(3) . . . . ? C1 Sb1 C20 O2 -2.2(3) . . . . ? C1 Sb1 C20 C21 173.7(2) . . . . ? O2 C20 C21 C22 -114.6(3) . . . . ? Sb1 C20 C21 C22 69.2(3) . . . . ? O2 C20 C21 C26 76.5(4) . . . . ? Sb1 C20 C21 C26 -99.7(3) . . . . ? C26 C21 C22 C23 10.5(5) . . . . ? C20 C21 C22 C23 -158.2(3) . . . . ? C26 C21 C22 C27 -165.4(3) . . . . ? C20 C21 C22 C27 25.9(5) . . . . ? C21 C22 C23 C24 -4.0(5) . . . . ? C27 C22 C23 C24 172.3(3) . . . . ? C22 C23 C24 C25 -4.6(5) . . . . ? C22 C23 C24 C31 176.1(3) . . . . ? C23 C24 C25 C26 6.9(5) . . . . ? C31 C24 C25 C26 -173.8(3) . . . . ? C24 C25 C26 C21 -0.5(5) . . . . ? C24 C25 C26 C35 -177.3(3) . . . . ? C22 C21 C26 C25 -8.4(5) . . . . ? C20 C21 C26 C25 160.4(3) . . . . ? C22 C21 C26 C35 168.1(3) . . . . ? C20 C21 C26 C35 -23.1(5) . . . . ? C23 C22 C27 C28 -159.6(3) . . . . ? C21 C22 C27 C28 16.3(5) . . . . ? C23 C22 C27 C30 -41.7(4) . . . . ? C21 C22 C27 C30 134.2(3) . . . . ? C23 C22 C27 C29 76.4(4) . . . . ? C21 C22 C27 C29 -107.7(4) . . . . ? C23 C24 C31 C32 -57.8(4) . . . . ? C25 C24 C31 C32 122.9(3) . . . . ? C23 C24 C31 C33 62.6(4) . . . . ? C25 C24 C31 C33 -116.7(4) . . . . ? C23 C24 C31 C34 -177.8(3) . . . . ? C25 C24 C31 C34 2.9(5) . . . . ? C25 C26 C35 C36 109.2(3) . . . . ? C21 C26 C35 C36 -67.3(4) . . . . ? C25 C26 C35 C38 -127.5(3) . . . . ? C21 C26 C35 C38 56.0(4) . . . . ? C25 C26 C35 C37 -8.3(4) . . . . ? C21 C26 C35 C37 175.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.96(5) 1.61(5) 2.565(3) 172(5) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.529 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.082 #===end